Calibration of Glassware (Laboratory)- Procedure

Standard Operating Procedure (SOP) and Protocol for Calibration of Laboratory Glassware (Class A)  like- Volumetric flask, Pipette calibration, Burette calibration used in Quality Control Laboratory for analysis purpose.

Glassware Calibration Procedure

1.0   Purpose:

    • The purpose of this SOP is to describe the procedure for calibration of laboratory glassware.

2.0   Scope:

    • This SOP is applicable for calibration of laboratory glassware used in Quality Control Laboratory.

3.0   References:

    • IP-2020; 2.1.6. Volumetric GlasswareCalibration of Glassware
    • Manufacturer COA

4.0   Responsibilities:

    • Analyst:

    • To prepare the SOP.
    • To receive and calibrate the glassware as per procedure.
    • QC Head or designee:

    • To check the SOP.
    • Impart training to all concerned persons before implementations of SOP.
    • To ensure proper maintenance of respective documents.
    • Quality Assurance:

    • To check the SOP.
    • To ensure that implementation of system is as per SOP.

5.0   Procedure for Glassware Calibration:

    • General Procedure:
    • Review the manufactures certificates and put a review stamp on it.
    • To select the glassware (volumetric flask, pipette, burette) for calibration from fresh consignment or as and when required according to √ n+1 method.
    • If the calibration of the above is not within the limit, the consignments shall be returned to party.
    • Numbering of glassware shall be marked as follows :

QC/CAL/Z/YY/XXX

where,

QC   = Quality Control

CAL  = Calibration

Z  =  F (Volumetric Flask), P (Pipette), B (Burette)

YY   = Last two digit of year (eg;12, for year 2012)

XXX = serial number of glassware

    • Assign calibration ID No to each glassware which to be calibrated, accordingly.
    • Precautions during Glassware Calibration:

    • Handle glassware carefully.
    • Pipette/burette should be dried in vertical position and touched against wall of receiving vessel to drain the tips.
    • Use PPE’s such as nose mask, gloves etc. as per requirement during the handling of glassware.
    • Calculation:

%RSD    = 100/Xm x [Ʃ(Xi-Xm)²/n-1]½

Xm   = Mean value

Xi     = Individual value

n      = Number of analysis

  • Calibration Protocol & Procedure for Volumetric Flask (Glassware):

Glassware Name Template Issuance No.
Make ID No.
Nominal Volume Calibration date

Calibration Requirement:-

    • Balance                     Code No.______________    Valid upto _________
    • Digital Thermometer Code No.______________    Valid upto _________
    • Distilled water

Procedure for Volumetric Flask Calibration:-

    • Place the required amount of distilled water in beaker.
    • Allow the temperature of water to equilibrate to room temperature (250C ± 20C).
    • Weigh the dry empty flask on calibrated balance and note down the weight (W1
      Advertisement
      ).
    • Record the observed temperature of water before pouring in volumetric flask (T1).
    • Fill the flask to nominal volume with distilled water (25±2°C).
    • Weigh it again and note down the weight (W2).
    • After weighing again record the temperature (T2), the variation in temperature (ΔT) shall not be  more than ± 0.50C  from the initial temperature of water.
    • Calculate the weight difference (ΔW) between empty flask (W1) and flask with water (W2)
    • Convert weight difference in terms of ml by calculating the wt/ml of water.
    • Calculate the error in ml and percentage.
    • Repeat the above step in triplicate.
    • Calculate the observed volume and relative standard deviation. RSD shall be with in 1.0%.

Calculations:-

           Weight difference(gm), ΔW =  W2  –  W1                   

           Observed Volume (ml), VObserve =   ΔW/ D

Volume Difference(ml),ΔV  =  VNominal – VObserve

ΔV                           

Relative Error (%)  =  —————— X 100                    

VNominal                                                  

where,

W1 = Weight of empty flask                                  VNominal = Nominal Volume

W2 = Weight of flask filled with water                 VObserve = Observe Volume

D = Density of water at 25 0C (0.997 g/ml)

Observations:-

Sr.

No.

Water Temp.

(OC)

Temp.Diff

ΔT(OC)

Flask Weight

(gm)

Weight Diff.

ΔW (gm)

Observe Vol.(ml) Vol. Diff. ΔV (ml) Relative Error (%)             
 Before Weight (T1)  After

Weight

(T2)

T2 – T1

 

Empty

W1

Filled

W2

W2 – W1 VObserve

=  ΔW/D

 

VNominal – VObserve ΔV/VNominal x 100
Mean
Limit: NMT 1%
 %RSD

Acceptance Criteria:

Nominal Volume(ml) 5 10 20 25 50 100 200 250 500 1000
Class A Tolerance (± ml) 0.02 0.02 0.04 0.03 0.04 0.06 0.15 0.1 0.15 0.2
Relative Error (± %) 0.4 0.2 0.2 0.12 0.08 0.06 0.08 0.04 0.03 0.02
  • Calibration Protocol & Procedure for Pipette (Glassware):

Glassware Name Template Issuance No.
Make ID No.
Nominal Volume Calibration date

Calibration Requirements:-

    • Balance Code No.______________    Valid upto _________
    • Digital Thermometer Code No.______________    Valid upto _________
    • Distilled water

Procedures for Pipette Calibration:-

    • Place the require amount of distilled water in beaker.
    • Allow the temperature of water to equilibrate to room temperature (250C ± 20C)
    • Weigh the dry empty beaker on calibrated balance and note down the weight (W1).
    • Record the observed temperature of water before pouring in pipette (T1).
    • Fill the pipette to nominal volume with distilled water (25±2°C).
    • Transfer the filled volume to beaker, weigh it again and note down the weight (W2).
    • After weighing, again record the temperature (T2), the variation in temperature (ΔT) shall not be more than ± 0.50C from the initial temperature of water.
    • Calculate the weight difference (ΔW).
    • Convert weight difference in terms of ml by calculating the wt/ml of water.
    • Calculate the error in ml and percentage.
    • Repeat the above step in triplicate.
    • Calculate the observed volume and RSD shall be within1.0%

Calculations :-

Weight difference(gm), ΔW =  W2  –  W1                      where,  

         Observed Volume (ml), VObserve =   ΔW/ D                 VNominal  =  Nominal Volume

Volume Difference(ml),ΔV  =  VNominal – VObserve         VObserve = Observe Volume

ΔV                                            W= Weight of empty beaker

Relative Error (%)  =  ——– X 100                      W2  = Weight of beaker filled with water

VNominal                                                 D = Density of water at 25 0C (0.997 g/ml)

Observations:-

Sr.

No.

Water Temp.

(OC)

Temp.Diff

ΔT(OC)

Beaker Weight

(gm)

Weight Diff.

ΔW (gm)

Observe Vol.(ml) Vol. Diff. ΔV (ml) Relative Error (%)                             
 Before Weight (T1)  After

Weight

(T2)

T2 – T1

 

Empty

W1

Filled

W2

W2 – W1 VObserve

=  ΔW/D

 

VNominal – VObserve ΔV/VNominal x 100
Mean
Limit: NMT 1% % RSD

 Acceptance Criteria:

Nominal Volume (ml) 1 2 5 10 20 25 50 100
Class A One Mark Pipettes
 Tolerance (± ml) 0.01 0.01 0.02 0.02 0.03 0.03 0.04 0.06
Relative Error (± %) 1 0.5 0.4 0.2 0.15 0.12 0.08 0.06
Class A Graduated Pipettes
Subdivision (ml) 0.01 0.02 0.05 0.1 0.2
Tolerance (± ml) 0.006 0.01 0.03 0.05 0.1
Relative Error (± %) 0.6 0.5 0.6 0.5 0.4

 

Nominal Volume (ml) 3 4 6 9 15
Class A One Mark Pipettes
 Tolerance (± ml) 0.01 ±0.01 0.01 0.02 0.03
Relative Error (± %) 0.3 0.3 0.2 ±0.2 0.2
  • Calibration Protocol & Procedure for Burette (Glassware):

Glassware Name Template Issuance No.
Make ID No.
Nominal Volume Calibration date

Calibration Requirements:-

    • Balance  Code No.______________    Valid upto _________
    • Digital Thermometer Code No.______________    Valid upto _________
    • Distilled water

Procedures for Burette Calibration :-

    • Place the require amount of distilled water in beaker. Allow the temperature of water to equilibrate to room temperature (250C ± 20C)
    • Take the weight of empty beaker (W1).
    • Record the observed temperature of water before pouring in pipette (T1).
    • Fill the burette to nominal volume with distilled water (25±2°C).
    • Transfer the volume to beaker, weigh it again and note down the weight (W2).
    • After weighing, again record the temperature (T2), the variation in temperature (ΔT) shall not be more than ± 0.50C from the initial temperature of water.
    • Calculate the weight difference (ΔW).
    • Convert weight difference in terms of ml by calculating the wt/ml of water.
    • Calculate the error in ml and percentage.
    • Repeat the above step in triplicate.
    • Calculate the observed volume and relative standard deviation.
    • RSD shall be with in 1.0%.

Calculations:-

Weight difference(gm), ΔW =  W2  –  W1                      where,  

         Observed Volume (ml), VObserve =   ΔW/ D                 VNominal  =  Nominal Volume

Volume Difference(ml),ΔV  =  VNominal – VObserve         VObserve = Observe Volume

ΔV                                            W= Weight of empty beaker

Relative Error (%)  =  ——– X 100                      W2  = Weight of beaker filled with water

VNominal                                                 D = Density of water at 25 0C (0.997 g/ml)

Observations :-

Sr.

No.

Water Temp.

(OC)

Temp.Diff

ΔT(OC)

Beaker Weight

(gm)

Weight Diff.

ΔW (gm)

Observe Vol.(ml) Vol. Diff. ΔV (ml) Relative Error (%)
 Before Weight (T1)  After

Weight

(T2)

T2 – T1

 

Empty

W1

Filled

W2

W2 – W1 VObserve

=  ΔW/D

 

VNominal – VObserve ΔV/VNominal x 100
Mean
Limit: NMT 1% %RSD

Acceptance Criteria:

Nominal Capacity (ml) 10 (micro) 25 50 100
Subdivision (ml) 0.05 0.05 0.1 0.1
Class A Tolerance (± ml) 0.01 0.03 0.05 0.1
Relative Error (± %) 0.1 0.12 0.1 0.1

Attachment : Volumetric flask calibration log book

Sr. No

Receiving date Date of calibration Nominal volume Calibration ID Calibrated By

Checked By

Attachment : Pipette calibration log book

Sr. No

Receiving date Date of calibration Nominal volume Calibration ID Calibrated By

Checked By

Attachment : Burette calibration log book

Sr. No

Receiving date Date of calibration Nominal volume Calibration ID Calibrated By

Checked By

Attachment : Template issuance log book

Sr. No

Date of issuance Protocol issuance No Glassware/

Volume

Glassware code No Glassware calibration ID No Issued By Received By

Remark

 

pharmabeginers

Janki Singh is experienced in Pharmaceuticals, author and founder of Pharma Beginners, an ultimate pharmaceutical blogging platform. Email: [email protected]

Leave a Reply